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目的:建立高效分子排阻色谱(HPSEC)法测定头孢尼西钠中的聚合物,并与葡聚糖凝胶G~(-1)0为填料的凝胶色谱法进行比较。方法:HPSEC法采用表面键合亲水薄膜硅胶为填料的色谱柱(Zenix SEC~(-1)50,7.8 mm×300 mm);流动相为0.01mol·L~(-1)磷酸盐缓冲液-乙腈(95∶5);流速:1.0mL·min~(-1);检测波长250 nm。结果:HPSEC法:头孢尼西及其聚合物分别在1~100μg·mL~(-1)和0.25~1.75 mg·mL~(-1)范围内的线性关系良好,头孢尼西的定量限为1.0ng·mL~(-1),精密度(RSD)为0.57%,聚合物测定重复性(RSD)为1.01%。凝胶色谱法:头孢尼西的定量限为500 ng·mL~(-1),精密度(RSD)为1.81%,聚合物测定重复性(RSD)为3.08%。HPSEC和凝胶色谱法测得的样品中头孢尼西聚合物的量分别为1.31%和0.23%。结论:HPSEC法适于测定头孢尼西钠聚合物,较凝胶色谱法专属性强,灵敏度高,重复性好,操作简便。
OBJECTIVE: To establish a high performance liquid chromatography (HPLC) method for the determination of polymers in cefonicid sodium and to compare it with gel chromatography using dextran gel G ~ (-1) 0 as a filler. Methods: HPSEC was performed on Zenix SEC (-1) 50, 7.8 mm × 300 mm column with hydrophilic silica membrane as the surface layer. The mobile phase consisted of 0.01 mol·L -1 phosphate buffer - acetonitrile (95: 5); flow rate: 1.0 mL · min -1; detection wavelength 250 nm. Results: The linear relationship between cefonicid and its polymer in the range of 1 ~ 100μg · mL -1 and 0.25 ~ 1.75 mg · mL -1 were good. The limit of quantitation of cefonicid was 1.0 ng · mL -1, RSD was 0.57%, and polymer repeatability (RSD) was 1.01%. Gel chromatography: The limit of quantification of cefonicid was 500 ng · mL -1, the precision (RSD) was 1.81%, and the polymer repeatability (RSD) was 3.08%. The amount of cefonicid polymer in the samples measured by HPSEC and gel chromatography were 1.31% and 0.23%, respectively. Conclusion: The HPSEC method is suitable for the determination of cefonicid sodium polymer, which is more specific, sensitive and reproducible than gel chromatography.